食品及环境样品中三聚氰胺的液质联用分析技术分析-analysis of melamine in food and environmental samples by liquid chromatography-mass spectrometry.docxVIP

南昌航空 南昌航空大学硕士学位论文 摘要 II II 水样中三聚氰胺和灭蝇胺的萃取效果，探索出 PCX 柱可同时高效萃取水样中三聚 氰胺和灭蝇胺，提出了以氰基柱（-CN）为分析柱和以一级质谱特征离子（三聚氰 胺 m/z127，灭蝇胺 m/z167）进行定量的同时检测的分析方法。所建立的方法已成 功用于南昌市区及周边湖水、河水、江水等不同实际水样中三聚氰胺的检测。结 果表明，三聚氰胺在天然水样中普遍存在。 5、以高效液相色谱法定量测定三聚氰胺为基础，研究了蜜胺餐具（碗） 在微波加热使用条件下向食品模拟物中迁移的三聚氰胺量。系统考察了模拟溶剂 的类型、微波辐射功率、微波辐射时间等条件对三聚氰胺迁移量的影响。结果表 明，蜜胺碗在以 4%乙酸为食品模拟物时，经中高火微波加热 5 分钟后，三聚氰胺 的迁移量超出国家标准规定的最大允许量。中高火微波加热盛有酸性溶剂的蜜胺 碗，不仅会迁移出较高含量的三聚氰胺，而且会迁移出多种其它组分，证实了其 原因与碗内表面结构遭到破坏有关。 关键词：三聚氰胺；固相萃取；分子印迹固相萃取；微波辅助萃取；高效液相色 谱/质谱联用；环境水样；蜜胺餐具 III III Abstract With the development of society, people pay more attention to pollution on food safety. After the case of “pet food in USA” and “Sanlu milk in china”, The analytical technique of melamine and other toxic and harmful pollutants in environment field has become a hotspot of analytical chemistry research. Since low content of melamine in food and environment, complex matrix, and high sensitive, high selective is required, high performance liquid chromatography (HPLC) and liquid chromatography-mass spectrometry (LC-MS) are become important method for melamine analysis. But, the difficulty is the development of a fast and reliable pretreatment method to real sample. This paper described molecularly imprinted solid phase extraction for determination of melamine in milk samples and microwave-assisted extraction for determination of melamine in egg samples. In addition, the melamine content in environmental water samples and melamine bowl under microwave irradiation were investigated. This thesis includes the following five parts: This section firstly introduces the characteristics and source, the dangers, the cases and current detection methods for melamine. Secondly, description of the development and application of LC/MS for melamine analysis in environmental and food samples. Then, introduction of the molecularly imprinted solid phase extraction and microwave-assisted extraction. Finally, description of the purposes and contents for the thesis. A molecularly imprint